A method and an apparatus for treating plant based raw material with an enzymatic hydrolysis

ABSTRACT

The invention relates to a method and an apparatus for treating plant based raw material with an enzymatic hydrolysis, in which the plant based raw material (1) is treated to form lignocellulosic material (3a,3b) and the lignocellulosic material (3a,3b) or its fraction (10) is conducted into the enzymatic hydrolysis (4), wherein the method comprises at least one treatment stage (2a,2b,2c) in which the plant based raw material (1) is treated so that the lignocellulosic material (3a,3b) contains over 80% fine solid particles which are fiber-like or indefinable particles smaller than 0.2 mm, defined by an optical measurement device, the lignocellulosic material (3a,3b) or at least one fraction (10) of the lignocellulosic material is supplied into the enzymatic hydrolysis (4) for forming a lignin based material (5), and at least one solid-liquid separation stage (6) after the enzymatic hydrolysis (4) in which a lignin fraction (7) and a soluble carbohydrate containing fraction (8) are separated. Further, the invention relates to the soluble carbohydrate containing fraction, the lignin fraction, the lignin based material, the liquid fraction and the solid fraction, and their uses.

FIELD OF THE INVENTION

The invention relates to a method and an apparatus for treating plantbased raw material with an enzymatic hydrolysis. Further, the inventionrelates to a soluble carbohydrate containing fraction and its use.Further, the invention relates to a lignin fraction and its use.

BACKGROUND OF THE INVENTION

Known from prior art is different methods for forming carbohydrates andlignin from different raw materials, such as biomass. Many bio-refineryprocesses, e.g. hydrolysis, generate lignin and sugars after thetreatment of the biomass.

OBJECTIVE OF THE INVENTION

The objective of the invention is to disclose a new method for producinga lignin fraction and a soluble carbohydrate containing fraction.Another objective of the invention is to produce a pure lignin fraction.Another objective of the invention is to produce a lignin fraction andsoluble carbohydrate containing fraction effectively. Another objectiveof the invention is to improve an enzymatic hydrolysis process.

SUMMARY OF THE INVENTION

The method for treating plant based raw material with an enzymatichydrolysis according to the present invention is characterized by whatis presented in claim 1.

The apparatus for treating plant based raw material with an enzymatichydrolysis according to the present invention is characterized by whatis presented in claim 17.

The soluble carbohydrate containing fraction according to the presentinvention is characterized by what is presented in claim 23.

The lignin fraction according to the present invention is characterizedby what is presented in claim 24.

The lignin based material according to the present invention ischaracterized by what is presented in claim 25.

The liquid fraction according to the present invention is characterizedby what is presented in claim 26.

The solid fraction according to the present invention is characterizedby what is presented in claim 27.

The use of the soluble carbohydrate containing fraction according to thepresent invention is characterized by what is presented in claim 28.

The use of the lignin fraction according to the present invention ischaracterized by what is presented in claim 29.

The use of the lignin based material according to the present inventionis characterized by what is presented in claim 30.

The use of the liquid fraction according to the present invention ischaracterized by what is presented in claim 31.

The use of the solid fraction according to the present invention ischaracterized by what is presented in claim 32.

The use of the liquid mixture according to the present invention ischaracterized by what is presented in claim 33.

BRIEF DESCRIPTION OF THE DRAWINGS

The accompanying drawings, which are included to provide a furtherunderstanding of the invention and constitutes a part of thisspecification, illustrate some embodiments of the invention and togetherwith the description help to explain the principles of the invention. Inthe drawings:

FIG. 1 is a flow chart illustration of a method according to oneembodiment of the present invention,

FIG. 2 is a flow chart illustration of a method according to anotherembodiment of the present invention,

FIG. 3 is a flow chart illustration of a method according to anotherembodiment of the present invention,

FIG. 4 is a flow chart illustration of a method according to anotherembodiment of the present invention, and

FIG. 5 shows results from a viscosity measurement of the lignocellulosicmaterial according to one method embodiment of the present invention.

DETAILED DESCRIPTION OF THE INVENTION

In a method for treating plant based raw material (1) with an enzymatichydrolysis (4), the plant based raw material (1) is treated to formlignocellulosic material (3 a,3 b), and the lignocellulosic material (3a,3 b) or its fraction (10) is conducted into the enzymatic hydrolysis(4). The method comprises at least one treatment stage (2 a,2 b,2 c) inwhich the plant based raw material (1) is treated so that thelignocellulosic material (3 a,3 b) contains over 80% fine solidparticles which are fiber-like or indefinable particles smaller than 0.2mm, defined by an optical measurement device, e.g. by Metso FS5, and thelignocellulosic material (3 a,3 b) or at least one fraction (10) of thelignocellulosic material is supplied into the enzymatic hydrolysis (4)for forming a lignin based material (5). Further, the method comprisesat least one solid-liquid separation stage (6) after the enzymatichydrolysis (4) into which the lignin based material (5) is supplied andin which a lignin fraction (7) and a soluble carbohydrate containingfraction (8) are separated.

One embodiment of the method of the present invention is shown inFIG. 1. Another embodiment of the method of the present invention isshown in FIG. 2. Another embodiment of the method of the presentinvention is shown in FIG. 3. Another embodiment of the method of thepresent invention is shown in FIG. 4.

The apparatus comprises at least one treatment device (2 a,2 b,2 c) inwhich the plant based raw material (1) is treated to formlignocellulosic material (3 a,3 b) so that the lignocellulosic material(3 a,3 b) contains over 80% fine solid particles which are fiber-like orindefinable particles smaller than 0.2 mm, defined by an opticalmeasurement device, e.g. by Metso FS5, at least one enzymatic hydrolysisdevice (4) in which a lignin based material (5) is formed from thelignocellulosic material (3 a,3 b) or at least one fraction (10) of thelignocellulosic material, at least one solid-liquid separation device(6) after the enzymatic hydrolysis device in which a lignin fraction (7)and a soluble carbohydrate containing fraction (8) is separated fromlignin based material (5), and at least one feeding device for feedingthe plant based raw material (1) into the treatment device. The feedingdevice can be any feeding device, e.g. pump, screw, inlet means or othersuitable feeding device. Further, the apparatus can comprise means, suchas discharge means or outlet means, e.g. pipe, pipe fitting or assembly,for supplying the soluble carbohydrate containing fraction and ligninfraction out from the apparatus.

In this context, an enzymatic hydrolysis means any enzymatic hydrolysis.In one embodiment, the enzyuratic hydrolysis is an enzymatic hydrolysisof cellulose.

In this context, a soluble carbohydrate containing fraction (8) meansany soluble carbohydrate containing filtrate which is separated from thelignin based material (5) at the solid-liquid separation stage (6) afterthe enzymatic hydrolysis. In a preferred embodiment, the solublecarbohydrate containing fraction includes carbohydrates, preferably C6sugars (C₆H₁₂O₆ or (C₆(H₂O)_(n)). The soluble carbohydrate containingfraction may comprise carbohydrates, such as monosaccharides (C₆H₁₂O₆ orC₅H₁₀O₅), disaccharides (C₁₂H₂₂O₁₁), oligosaccharides and/orpolysaccharides ((C₆H₁₀O₅)_(n) or (C₅H₈O₄)_(n)). Preferably, the solublecarbohydrate containing fraction comprises soluble C6 carbohydrates(C₆H₁₂O₆ or C₆(H₂O)_(n)) and other soluble carbohydrates. The solublecarbohydrate containing fraction may comprise also other components.

In this context, a lignin fraction (7) means a solid residue, such as asolid cake, when the soluble carbohydrate containing filtrate has beenseparated from the lignin based material (5) at the solid-liquidseparation stage (6) after the enzymatic hydrolysis. In a preferredembodiment, the lignin fraction comprises lignin and carbohydrates,preferably solid C6 carbohydrates (C₆H₁₂O₆ or C₆(H₂O)_(n)). The ligninfraction may comprise also other carbohydrates and other components.Preferably, the lignin fraction is in the solid form.

In this context, lignin based material (5) means any lignin containingcomposition that can be in the form of slurry. The lignin based materialcontains soluble compounds, solid material and liquid, e.g. water. Inone embodiment, the lignin based material contains at least solublecarbohydrates and lignin. In one embodiment, the lignin based materialmay comprise also other solid carbohydrates and/or other components. Inone embodiment, the lignin based material can be pumped. In oneembodiment, the lignin based material contains free liquid, such as freewater. Preferably, the lignin based material has been formed from thelignocellulosic material (3 a,3 b), in one embodiment from solidfraction (10) of the lignocellulosic material (3 a,3 b). In oneembodiment, the lignin based material is a crude lignin slurry.

In this context, plant based raw material (1) means any plant based rawmaterial, e.g. wood based raw material and/or other plant basedmaterial. The plant based raw material includes lignin, cellulose andhemicellulose. In one embodiment, the plant based raw material isselected from the group consisting of wood based material, wood,lignocellulosic biomass, agricultural residues, bagasse based material,sugarcane bagasse, corn based material, corn stover, wheat straw, ricestraw, woody biomass, woody perennials, vascular plants and the like andtheir mixtures and their combinations. In one embodiment, the plantbased raw material comprises is wood based material or a mixturecomprising wood based material. In one embodiment, the plant based rawmaterial is wood based material or a mixture comprising wood basedmaterial. In one embodiment, the wood based material is selected fromhardwood, softwood or their combination. In one embodiment, the plantbased raw material comprises plant pieces, e.g. wood pieces.

In this context, lignocellulosic material (3 a,3 b) refers anylignocellulosic material which has been formed by treating, e.g.pretreating, from the plant based raw material by means of at least onesuitable treatment method in one or more steps. In one embodiment, thelignocellulosic material contains carbohydrates and lignin. Preferably,the carbohydrates have C_(n)(H₂O)_(n) or C_(n)(H₂O)_(n−1). Thecarbohydrates can comprise monosaccharides (C₆H₁₂O₆ or C₅H₁₀O₅),disaccharides (C₁₂H₂₂O₁₁), oligosaccharides and/or polysaccharides((C₆H₁₀O₅)_(n) or (C₅H₈O₄)_(n)). Preferably, the lignocellulosicmaterial includes carbohydrates, such as soluble C5 carbohydrates(C₅H₁₀O₅ or C₅(H₂O)_(n)) and solid C6 carbohydrates (C₆H₁₂O₆ orC₆(H₂O)_(n)). The lignocellulosic material may contain one or morelignocellulosic material components. In one embodiment, thelignocellulosic material is in the form of suspension which containsliquid, such as water.

The lignocellulosic material (3 a,3 b) is formed from the plant basedraw material (1) and is treated at the treatment stage, preferably inone or more treatment step (2 a,2 b,2 c). In one embodiment, thetreatment stage comprises at least one pretreatment step (2 a,2 b) whichis selected from the group consisting of physical treatment, such asmilling, extrusion, microwave treatment, ultrasound treatment and freezetreatment, chemical treatment, such as acid treatment, alkalinetreatment, ionic liquid treatment, organosolv treatment and ozonolysis,physico-chemical treatment, such as steam explosion treatment, ammoniafiber explosion treatment, CO₂ explosion treatment, liquid hot watertreatment and wet oxidation, biological treatment and theircombinations. Preferably, the plant based raw material is treated todissolve hemicellulose. In one embodiment, the lignocellulosic materialis formed or treated by the hydrolysis, e.g. acid hydrolysis,autohydrolysis, thermal hydrolysis, enzymatic hydrolysis, supercriticalhydrolysis and/or subcritical hydrolysis, in which at least a part oflignin is separated from the raw material in connection with thehydrolysis. In one embodiment, the lignocellulosic material is formed ortreated by the steam explosion, in which hemicelluloses are treated andin which at least a part of polysaccharides of the hemicellulosesdegrade into monosaccharides and oligosaccharides by means of ahydrolysis and in which pressure is rapidly released. In one embodiment,the lignocellulosic material is formed or treated by the hydrolysis andby the steam explosion in one or more steps. In one embodiment, thelignocellulosic material is formed or treated by the catalyticpretreatment, e.g. by using acid or base as catalyst. In thepretreatment process the plant based raw material enters the reactorunit where the pretreatment takes place. The lignocellulosic materialcan be treated by means of one or more pretreatment. In one embodiment,the treated lignocellulosic material can be blown to a blowtank. In oneembodiment, the lignocellulosic material can be dewatered, e.g. bydewatering presses in two stages. The dewatering makes possible toseparate sugar based streams.

In one embodiment, the plant based raw material (1) is treated by meansof a steam explosion treatment at the pretreatment step (2 a,2 b). Inone embodiment, the plant based raw material (1) is treated by means ofa steam explosion treatment in presence of a chemical agent at thepretreatment step. In one embodiment, the chemical agent is anon-alkaline agent. In one embodiment, the chemical agent is an acid. Inone embodiment, the chemical agent is a dilute acid, e.g. H₂SO₄. In oneembodiment, the chemical agent is H₂SO₄. In one embodiment, the chemicalagent may be any dilute acid. In one embodiment, pH of the dilute acidis between 1.5-2.5. In one embodiment, temperature is under 180° C. inthe steam explosion if water is used as a single solvent. In oneembodiment, temperature is between 170-210° C. in the steam explosion ifwater is used as a single solvent. In one embodiment, temperature is130° C. or over 130° C. in the steam explosion if ethanol is used as asolvent. In one embodiment, pressure is depending on temperature in thesteam explosion. In one embodiment, pressure is between 8-20 bar in thesteam explosion, especially if water is used as a single solvent. In oneembodiment, pH is between 1 4, in one embodiment 1-3, in one embodiment1-2, in connection with the steam explosion. In one embodiment, pH isbetween 1-4, in one embodiment 1-3, in one embodiment 1-2, in thehydrolysis in connection with the steam explosion. In one embodiment,the apparatus comprises a means for a steam explosion. By means of thedilute acid treatment and the steam explosion the most of thepolysaccharides of the hemicelluloses degrade into monosaccharides, andpartly into oligosaccharides, and almost all of hemicellulose can behydrolyzed by short residence time at typical conditions.

In one embodiment, the plant based raw material (1) is treated by meansof a hydrolysis and a mechanical treatment at the pretreatment steps (2a,2 b).

In one embodiment, the lignocellulosic material (3 a) is treated bymeans of a soaking (2 c) after the pretreatment step (2 a,2 b). In oneembodiment, the lignocellulosic material (3 a) is diluted for thesoaking (2 c), e.g. before and/or during the soaking. In one embodiment,the dry matter content of the lignocellulosic material (3 a) is adjustedfor the soaking, e.g. before and/or during the soaking, so that thelignocellulosic material comprises over 40% by weight liquid, in oneembodiment over 50% by weight liquid, in one embodiment over 60% byweight liquid, and in one embodiment over 70% by weight liquid. In oneembodiment, temperature is between 20-100° C., in one embodiment 20-90°C., in one embodiment 50-90° C., in one embodiment 50-80° C., in thesoaking. In one embodiment, the residence time is below 72 hours, in oneembodiment below 24 hours. In one embodiment, the residence time isbelow 12 hours, in one embodiment below 6 hours, in one embodiment below3 hours, and in one embodiment below 2 hours. In one embodiment, theresidence time is over 15 min, in one embodiment over 30 min, and in oneembodiment over 45 min. In one embodiment, the apparatus comprises asoaking device. By means of the soaking good recovery of thehemicellulose can be achieved.

In one embodiment, the lignocellulosic material (3 a,3 b) or its solidfraction (10), preferably material which is supplied to the enzymatichydrolysis (4), consists of fine solid particles. Particle size of thelignocellulosic material or its solid fraction can be measured with anoptical measurement device, such as Metso FS5 or Coulter LS230. In oneembodiment, the lignocellulosic material (3 a,3 b) or its solid fraction(10) contains over 85%, in one embodiment over 90%, in one embodimentover 92%, and in one embodiment over 94%, fine solid particles, definedby an optical measurement device, such as by Metso FS5. The fine solidparticles can be fiber-like or indefinable particles smaller than 0.2mm. In one embodiment, the lignocellulosic material (3 a,3 b) or itssolid fraction (10) contains fine solid particles from which over 85%,in one embodiment over 90%, in one embodiment over 92%, and in oneembodiment over 94%, are smaller than 0.2 mm, defined by Metso FS5. Inone embodiment, the lignocellulosic material (3 a,3 b) or its solidfraction (10) contains fine solid particles which are particles that aresmall enough to pass through the Bauer McNett 200-mesh screen. In oneembodiment, the lignocellulosic material (3 a,3 b) or its solid fraction(10) comprises fine solid particles which have particle size Modebetween 18-300 μm, defined by Coulter LS230. In one embodiment, thelignocellulosic material (3 a,3 b) or its solid fraction (10) comprisesfine solid particles which have Coulter LS Particle size Mode 19-200 μm,in one embodiment 20-150 μm, in one embodiment 20 120 μm, and in oneembodiment 21-75 μm, defined by Coulter LS230. The values for particlesize are depending on the method and thus values from Metso FS5 andCoulter LS230 and Bauer McNett cannot be directly compared. Particlesize of the solid particles can be defined based on ISO 16065-N or TAPPIT271. The pretreatment process decreases the particle size and fibrelength of original wood fibre, which can be defined by separating fibresby cooking the wood in e.g. sulphate process or maceration. The sulphateprocess is resulting fibre length of about 80% of the one after themaceration.

In one embodiment, the viscosity of the lignocellulosic material (3 a,3b) or its fraction (10), preferably material which is supplied to theenzymatic hydrolysis (4), is below 18000 mPas, in one embodiment below13000 mPas, in one embodiment below 10000 mPas, and in one embodimentbelow 8000 mPas, at 15% dry matter content, measured by Brookfieldviscosity device at 45° C. with 10 rpm and spindel type “Vane”. In thiscontext, the lignocellulosic material or its fraction comprises below 20w-% soluble matter during the viscosity measurement. By means of thesuitable viscosity the separation and the enzymatic hydrolysis can beimproved.

In one embodiment, the lignocellulosic material (3 a,3 b) or its solidfraction (10) contains over 80% fine solid particles which arefiber-like or indefinable particles smaller than 0.2 mm, defined by anoptical measurement device, e.g. by Metso FS5, and the viscosity of thelignocellulosic material (3 a,3 b) or its fraction (10) is below 18000mPas at 15% dry matter content, measured by Brookfield viscosity deviceat 45° C. with 10 rpm and spindel type “Vane”. In one embodiment, thelignocellulosic material (3 a,3 b) or its solid fraction (10) comprisesfine solid particles which have particle size Mode between 18-300 μm,defined by Coulter LS230, and the viscosity of the lignocellulosicmaterial (3 a,3 b) or its fraction (10) is below 18000 mPas at 15% drymatter content, measured by Brookfield viscosity device at 45° C. with10 rpm and spindel type “Vane”. In one embodiment, the viscosity of thelignocellulosic material (3 a,3 b) or its fraction (10) is below 18000mPas, in one embodiment below 13000 mPas, in one embodiment below 10000mPas, and in one embodiment below 8000 mPas, at 15% dry matter content,measured by Brookfield viscosity device at 45° C. with 10 rpm andspindel type “Vane”. In one embodiment, the lignocellulosic material (3a,3 b) or its solid fraction (10) contains over 85%, in one embodimentover 90%, in one embodiment over 92%, and in one embodiment over 94%,fine solid particles which are fiber-like or indefinable particlessmaller than 0.2 mm, defined by Metso FS5. In one embodiment, thelignocellulosic material (3 a, 3 b) or its solid fraction (10) comprisesfine solid particles which have Particle size Mode 19-200 μm, in oneembodiment 20-150 μm, in one embodiment 20 120 μm, and in one embodiment21-75 μm, defined by Coulter LS230.

In one embodiment, dry matter content of the lignocellulosic material (3a,3 b) is 20-80% by weight, in one embodiment 30-70% by weight, in oneembodiment 50-60% by weight, after the pretreatment (2,2 b) and/orsoaking (2 c). The dry matter content is determined at 45° C. by meansof evaporating. When the determination of the dry matter content is madeat temperature 45° C. so also small-molecular organic compounds remainin the mass during the drying of the determination. In one embodiment,the determination of the dry matter content may be done so that it isbased, at least partly or as applied, on NREL (National renewable energylaboratory) Laboratory Analytical Procedures for standard biomassanalysis determined in the Technical Report NREL/TR-510-48087 (revisedJuly 2011).

In one embodiment, the lignocellulosic material (3 a,3 b) is dilutedwith liquid, preferably with water or a filtrate from a separation, orsteam to form the feed to the separation stage (9) or the enzymatichydrolysis (4). In one embodiment, feed concentration of thelignocellulosic material (3 a,3 b) is 2-60% by weight, in one embodiment5-30% by weight, in one embodiment 10-20% by weight. If feedconcentration of the lignocellulosic material is low so then size of thedevice increases, for example at the separation stage (9).

In one embodiment, pH is adjusted before the enzymatic hydrolysis (4).In one embodiment, the pH is between 4.0-6.0. Preferably, pH valuedepends on an enzyme.

In one embodiment, the lignocellulosic material (3 a,3 b) is conducted asolid-liquid separation stage (9) in which a liquid fraction (11) and asolid fraction (10) are separated before the enzymatic hydrolysis, andthe solid fraction (10), in one embodiment at least a part of the solidfraction (10), is conducted into the enzymatic hydrolysis (4). Theapparatus comprises at least one solid-liquid separation device forseparating a liquid fraction (11) and a solid fraction (10). In oneembodiment, a washing filtrate or liquid fraction or a part of theliquid fraction from the separation stage (9) is recirculated to thelignocellulosic material (3 a) for the soaking (2 c), e.g. before and/orduring the soaking, and/or to the lignocellulosic material (3 b) beforethe solid-liquid separation stage (9) in order to dilute thelignocellulosic material.

The separation stage (9) before the enzymatic hydrolysis may be carriedout by means of a similar separation method or device as used in theseparation stage (6) after the enzymatic hydrolysis or by means of othersuitable separation method or device.

In this context, a liquid fraction (11) means any liquid fraction whichis separated from the lignocellulosic material (3 a,3 b) at anysolid-liquid separation stage (9) before the enzymatic hydrolysis. In apreferred embodiment, the liquid fraction includes carbohydrates,preferably C5 sugars (C₅H₁₀O₅ or (C₅(H₂O)_(n)). The liquid fraction maybe comprise carbohydrates, such as monosaccharides (C₆H₁₂O₆ or C₅H₁₀O₅),disaccharides (C₁₂H₂₂O₁₁), oligosaccharides and/or polysaccharides((C₆H₁₀O₅)_(n) or (C₅H₈O₄)_(n)). Preferably, the liquid fractioncomprises soluble C5 carbohydrates (C₅H₁₀O₅ or C₅(H₂O)_(n)) and othercarbohydrates. The liquid fraction may comprise also other components.

In this context, a solid fraction (10) means any solid fraction which isseparated from the lignocellulosic material (3 a,3 b) at anysolid-liquid separation stage (9) before the enzymatic hydrolysis. In apreferred embodiment, the solid fraction comprises carbohydrates, andpreferably solid C6 carbohydrates (C₆H₁₂O₆ or C₆(H₂O)_(n)), and lignin.The solid fraction may comprise also other carbohydrates and othercomponents.

The solid-liquid separation stage (6,9) may comprise one or moreseparation steps. In one embodiment, the solid-liquid separation iscarried out in one or more separation steps in the separation stage. Inone embodiment, the solid-liquid separation stage comprises more thanone sequential separation steps. In one embodiment, the solid-liquidseparation stage comprises different procedures which may be done inseparate separation steps. Alternatively, more than one procedure isdone in one process step.

In one embodiment, the method comprises more than one separation stages(6,9). In one embodiment, the method comprises more than one sequentialseparation stages. In one embodiment, the apparatus comprises more thanone separation devices. In one embodiment, the solid-liquid separationstage comprises at least one separation device. In one embodiment, thesolid-liquid separation stage comprises more than one separation device.In one embodiment, one or more separation steps can be done in the sameseparation device. In one embodiment, the separation device comprisesone or more separation step, e.g. separation segment.

In one embodiment, the separation device is based on a countercurrentwashing. In one embodiment, the separation device is selected from thegroup consisting of filtration device, centrifugal device and theircombinations. In one embodiment, the separation device is selected fromthe group consisting of pressure filtration device, vacuum filtrationdevice, filtration device based on underpressure, filtration devicebased on overpressure, filter press, other suitable press, centrifugaldevice and their combinations. In one embodiment, the separation deviceis a pressure filtration device, vacuum filtration device, filtrationdevice based on underpressure or filtration device based onoverpressure. Alternatively, the separation device can be anotherwashing device in which low amount of washing water is used and washingis done in high dry matter content. Then good recovery can be achieved.

In one embodiment, the separation is based on filtration, centrifugaltreatment or their combination. In one embodiment, the filtration iscarried out by pressure, underpressure or overpressure.

In one embodiment, the solid-liquid separation stage (6,9) comprises afiltration in which the soluble carbohydrate containing fraction orliquid fraction is separated in a liquid form and a solid cake isformed. Preferably, pressure is used in the filtration. In oneembodiment, liquid is separated by a pressure difference, such as bymeans of vacuum or overpressure. In one embodiment, the solid-liquidseparation stage comprises a washing in which a displacement washing ofthe lignocellulosic material is carried out with small amount cleanwater in order to remove majority of sugars, inhibitors and othersoluble compounds from the solid lignocellulosic material and to providehigh recovery of soluble compounds. Preferably, ratio of washing waterto solid is below 6, preferably below 3 and more preferably below 1.5.In one embodiment, the solid-liquid separation stage comprises thefiltration and washing. In one embodiment, the filtration and washing iscarried out in a static chamber, preferably in a non-moving chamber. Inone embodiment, the filtration and washing is carried out in one deviceunder pressure without mixing between the filtration and washing.Preferably, said separation device comprising the filtration and washingis in the vertical or horizontal plane, not in the inclined plane. Highconcentration and recovery of soluble material in the liquid phase canbe achieved with small amount of clean water, and a solid fractionwithout soluble compounds can be achieved.

In one embodiment, the separation is made by means of pressurefiltration. In one embodiment, the apparatus comprises at least onepressure filtration device as the solid-liquid separation device. In oneembodiment, the solid-liquid separation stage comprises one pressurefiltration device. In one embodiment, the solid-liquid separation stagecomprises more than one pressure filtration device. In a preferredembodiment, the washing in the pressure filtration device is based on adisplacement of liquid. In one embodiment, the pressure filtrationcomprises a pumping step, pressing, washing step, pressing and removalof a cake. In the pumping step, the solid cake is formed and pressed.Preferably, in the pumping step, a chamber of the pressure filtrationdevice is filled, and prepressing is made. In one embodiment, air blowis made after the pumping step or after the first pressing step tofurther remove liquid from the cake. Preferably, the solublecarbohydrate containing fraction or liquid fraction is separated inconnection with the pumping step. In the washing step, washing water ispressed through the cake and the cake is pressed and preferablydewatered. In the washing step, the liquid of the cake can be displacedby water. In one embodiment, air blow is made in the washing step tofurther remove liquid from the cake. The washing filtrate is separatedby pressing in connection with the washing step. The dewatered solidcake is removed from the pressure filtrate device. Preferably, thedewatered solid cake forms a solid fraction or lignin fraction. Anadvantage of the pressure filtration is that all separation steps can becarried out by one device.

In different separation stages the separation can be carried out bymeans of similar or different separation methods or separation devices.

In one embodiment, the lignin based material is diluted with liquid,preferably with water, or steam to form the feed to the separation stage(6). In one embodiment, feed concentration of the lignin based material(5) is 2-60% by weight, preferably 5-40% by weight, more preferable10-30% by weight, into the solid-liquid separation stage (6). If feedconcentration of the lignin based material is low so then size of thedevice increases. In one embodiment, the washing filtrate which isrecovered may be used in a dilution of the lignin based material.

In one embodiment, the lignocellulosic material (3 a,3 b) or itsfraction (10) or lignin based material (5) is fed by means of a pump,e.g. a mono pump or piston pump or other suitable pump, or othersuitable feeding device into the solid-liquid separation stage (9,6).Selection of the pump or feeding device is based on e.g. feedconcentration and/or viscosity of the lignocellulosic material or ligninbased material.

Preferably, at least a part of the soluble carbohydrate containingfraction (8) is supplied out from the separation stage (6) after theenzymatic hydrolysis. The soluble carbohydrate containing fraction canbe supplied out after any desired step of the separation stage. In oneembodiment, the soluble carbohydrate containing fraction is supplied outafter one or more step of the separation stage. The soluble carbohydratecontaining fractions may be combined or used separately as component.

Preferably, a lignin fraction (7) comprising solids is supplied out fromthe solid-liquid separation stage (6) after the enzymatic hydrolysis. Inone embodinvent, the lignin fraction is supplied out after one or morestep of the separation stage, preferably in one step. In one embodiment,the lignin fraction is supplied out after the last step.

In one embodiment, at least a part of the liquid fraction (11) issupplied out from the separation stage (9) before the enzymatichydrolysis. The liquid fraction can be supplied out after any desiredstep of the separation stage. In one embodiment, the liquid fraction issupplied out after one or more step of the separation stage. The liquidfractions may be combined or used separately as component. In oneembodiment, a part of the liquid fraction is separated from thelignocellulosic material (3 a,3 b) in connection with the treatmentstage (2 a,2 b,2 c) in which the lignocellulosic material is formedand/or treated. In one embodiment, at least a part of the liquidfraction (11) is recirculated to the lignocellulosic material (3 a,3 b)before the separation stage (9) or for the soaking (2 c), e.g. beforeand/or during the soaking. An amount of fresh water can be decreased bymeans of the recirculation.

In one embodiment, a solid fraction (10) comprising solids is suppliedout from the solid-liquid separation stage (9) and is supplied into theenzymatic hydrolysis (4). In one embodiment, the solid fractioncomprises C6 carbohydrates, such as (C₆H₁₂O₆ or (C₆(H₂O)_(n)), othersolid carbohydrates and lignin, and some other compounds, such as someresidual soluble material. In one embodiment, the solid fraction is inthe form of a cake. In one embodiment, dry matter content of the cake is30-70% by weight, preferably 35-60% by weight, more preferably 50-60% byweight, after the solid-liquid separation stage (9). In one embodiment,dry matter content of the cake is 7-70% by weight, preferably 15-45% byweight, more preferably 25-35% by weight, after the solid-liquidseparation stage (9). In one embodiment, the solid fraction containssoluble compounds below 20%, preferably below 15%, more preferably below6% by weight, most preferably below 3% by weight, after the solid-liquidseparation stage (9), determined by a gravimetric washing method.

In one embodiment, the soluble carbohydrate containing fraction (8) isformed from the lignin based material (5). In one embodiment, thesoluble carbohydrate containing fraction can be used as component inmanufacturing a final product or can be treated or concentrated. In oneembodiment, the soluble carbohydrate containing fraction (8) comprisessoluble C6 carbohydrates, such as C₆H₁₂O₆ or C₆(H₂O)_(n), and othersoluble carbohydrates, lignin and some other compounds. The solublecarbohydrate containing fraction may contain also C5 carbohydrates.Preferably, the soluble carbohydrate containing fraction can containmonosaccharides, and oligosaccharides. Further, the soluble carbohydratecontaining fraction can contain also polysaccharides. In one embodiment,the soluble carbohydrate containing fraction contains galactose,glucose, mannose, arabinose, xylose, glucuronic acid and galacturonicacid. In one embodiment, the soluble carbohydrate containing fractioncontains glucose more than xylose. Total carbohydrate content can bemeasured with HPLC after acid hydrolysis according to standard SCAN-CM71:09. Monomeric carbohydrate content can be measured with HPLC fromliquid composition directly without acid hydrolysis. In one embodiment,the total soluble concentrate of the soluble carbohydrate containingfraction is between 20 to 280 g/l, preferably between 40 to 240 g/l,more preferable between 55 to 210 g/l after the solid-liquid separation.In one embodiment, the total soluble concentrate of the solublecarbohydrate containing fraction is between 10 to 210 g/l, preferablybetween to 180 g/l, more preferable between 30 to 140 g/l after thesolid-liquid separation (6). In one embodiment, the total solubleconcentrate of the soluble carbohydrate containing fraction is between30 to 230 g/l, preferably between 50 to 220 g/l, more preferable between100 to 210 g/l after the solid-liquid separation. Preferably, thesoluble carbohydrate containing fraction is in the form of solution. Inone embodiment, carbohydrate concentrate of the soluble carbohydratecontaining fraction (8) is between 20 to 200 g/l, preferably between 40to 170 g/l, more preferable between 50 to 150 g/l after the solid-liquidseparation (6). In one embodiment, carbohydrate concentrate of thesoluble carbohydrate containing fraction is between 10 to 150 g/l,preferably between 20 to 125 g/l, more preferable between 30 to 100 g/lafter the solid-liquid separation. In one embodiment, carbohydrateconcentrate of the soluble carbohydrate containing fraction is between25 to 230 g/l, preferably between 50 to 215 g/l, more preferable between100 to 200 g/l after the solid-liquid separation.

In one embodiment, the lignin fraction (7) comprising solids is formedfrom the lignin based material (5). In one embodiment, the ligninfraction can be used as component in manufacturing a final product orcan be treated. In one embodiment, the lignin fraction (7) compriseslignin and solid C6 carbohydrates, such as (C₆H₁₂O₆ or (C₆(H₂O)_(n)),other solid carbohydrates and other solid components, and some othercompounds, such as some residual soluble material. In one embodiment,the lignin fraction is in the form of a cake. In one embodiment, drymatter content of the lignin fraction is 20-80% by weight. In oneembodiment, dry matter content of the lignin fraction is 30-60% byweight, preferably 40-60% by weight, more preferably 45-55% by weight,after the solid-liquid separation stage (6). In one embodiment, drymatter content of the lignin fraction is 7-70% by weight, preferably15-45% by weight, more preferably 30-40% by weight, after thesolid-liquid separation stage (6). The dry matter content is determinedat 60° C. by means of evaporating. In one embodiment, the determinationof the dry matter content may be done so that it is based, at leastpartly or as applied, on NREL (National renewable energy laboratory)Laboratory Analytical Procedures for standard biomass analysisdetermined in the Technical Report NREL/TR-510-48087 (revised July2011). In one embodiment, the cellulose content, i.e. glucan content, ofthe lignin fraction (7) is 3-70% by weight, preferably 5-60% by weightand more preferably 10-60% by weight, analyzed as glucose. In thiscontext, glucan means β-glucan, such as β-1,4-glucan, i.e. cellulose. Inone embodiment, the carbohydrate content of the lignin fraction (7) isbetween 2 to 50% by weight. In one embodiment, the carbohydrate contentis 10-30% by weight, and more preferably 15-25% by weight. In oneembodiment, the carbohydrate content is 40-70% by weight, and morepreferably 40-60% by weight. In one embodiment, the carbohydrate contentis 5-80% by weight, and more preferably 40-70% by weight. In oneembodiment, the lignin fraction (7) contains soluble compounds below 20%by weight, preferably below 15% by weight, more preferably below 6% byweight, most preferably below 3% by weight, after the solid-liquidseparation stage (6). In one embodiment, water soluble matter isdetermined by a gravimetric washing method.

In one embodiment the liquid fraction (11) is formed from thelignocellulosic material (3 a,3 b). In one embodiment, the liquidfraction can be used as component in manufacturing a final product orcan be treated or concentrated. In one embodiment, the liquid fraction(11) contains soluble C5 carbohydrates. The liquid fraction may containalso C6 carbohydrates, preferably below 20 w-%. Preferably, the liquidfraction can contain other monosaccharides, disaccharides,oligosaccharides and/or polysaccharides. In one embodiment, the liquidfraction contains galactose, glucose, mannose, arabinose, xylose,glucuronic acid and galacturonic acid. In one embodiment, the liquidfraction contains xylose more than glucose. In one embodiment, theliquid fraction contains glucose less than 20% by weight, in oneembodiment less than 15% by weight, less than 10% by weight, from anamount of the xylose. In one embodiment, the liquid fraction containsless than 50% by weight glucose and more than 50% by weight xylose, froman amount of the glucose and xylose. In one embodiment, a ratio (w/w) ofglucose to xylose, glucose:xylose, is less than 1. In one embodiment,the liquid fraction comprises soluble C5 carbohydrates, such as C₅H₁₀O₅or C₅(H₂O)_(n), and other carbohydrates and some other compounds. Totalcarbohydrate content can be measured with HPLC after acid hydrolysisaccording to standard SCAN-CM 71:09. Monomeric carbohydrate content canbe measured with HPLC from liquid composition directly without acidhydrolysis. In one embodiment, the soluble carbohydrate concentrate ofthe liquid fraction is over 50 g/l, preferably over 70 g/l, morepreferable over 100 g/l after the solid-liquid separation (9). In oneembodiment, the soluble carbohydrate concentrate of the liquid fractionis below 250 g/l, in one embodiment below 200 g/l, in one embodimentbelow 150 g/l after the solid-liquid separation. In one embodiment, thesoluble carbohydrate concentrate of the liquid fraction is between 15 to280 g/l, preferably 30 to 200 g/l, more preferable 50 to 165 g/l afterthe solid-liquid separation. Preferably, the liquid fraction is in theform of solution. In one embodiment, water soluble matter is between 20to 425 g/l, preferably 45 to 303 g/l, more preferable 75 to 250 g/lafter the solid-liquid separation (9). Water soluble matter can bedetermined by means of a method described later as “gravimetric washingmethod”.

In one embodiment, the soluble carbohydrate containing fraction (8) isrecovered. The soluble carbohydrate containing fraction may be used ascomponent in manufacturing a final product. In one embodiment, thesoluble carbohydrate containing fraction can be concentrated for furtheruse. In one embodiment, the soluble carbohydrate containing fraction issupplied to a further processing. In one embodiment, the monomerizationof the soluble carbohydrate containing fraction is made before thefurther processing. In one embodiment, the soluble carbohydratecontaining fraction is supplied to a fermentation process. In oneembodiment, the soluble carbohydrate containing fraction is used as asource material in fermentation. In one embodiment, the solublecarbohydrate containing fraction is supplied to a hydrolysis process. Inone embodiment, the soluble carbohydrate containing fraction is used asa source material in hydrolysis, e.g. acid hydrolysis or the like. Inone embodiment, the soluble carbohydrate containing fraction is suppliedto a chemical treatment. In one embodiment, the soluble carbohydratecontaining fraction is used as a source material in the chemicaltreatment. In one embodiment, the soluble carbohydrate containingfraction is supplied to a catalytic treatment. In one embodiment, thesoluble carbohydrate containing fraction is used as a source material inthe catalytic treatment. In one embodiment, the soluble carbohydratecontaining fraction is supplied to a polymerization process. In oneembodiment, the soluble carbohydrate containing fraction is used as asource material in the polymerization process. In one embodiment, thesoluble carbohydrate containing fraction is supplied to adepolymerization process. In one embodiment, the soluble carbohydratecontaining fraction is used as a source material in the depolymerizationprocess. In one embodiment, the soluble carbohydrate containing fractionis supplied to a degradation process. In one embodiment, the solublecarbohydrate containing fraction is used as a source material in thedegradation process. In one embodiment, the soluble carbohydratecontaining fraction is supplied to an enzymatic treatment. In oneembodiment, the soluble carbohydrate containing fraction is used as asource material in the enzymatic treatment. In one embodiment, thesoluble carbohydrate containing fraction is supplied to a manufacture ofbinder. In one embodiment, the soluble carbohydrate containing fractionis used as a source material in the manufacture of binder, e.g. woodbased binder. In one embodiment, the soluble carbohydrate containingfraction is supplied to a manufacture of food. In one embodiment, thesoluble carbohydrate containing fraction is used as a source material inthe manufacture of food. In one embodiment, the soluble carbohydratecontaining fraction is supplied to a manufacture of feed. In oneembodiment, the soluble carbohydrate containing fraction is used as asource material in the manufacture of feed. The soluble carbohydratecontaining fraction may be supplied directly to a fermentation,hydrolysis, chemical treatment, catalytic treatment, polymerizationprocess, depolymerization process, degradation process, enzymatictreatment, manufacture of binder, manufacture of feed, manufacture offood, or other suitable process or their combinations, or alternativelyvia a suitable treatment step or an additional step, e.g. additionalconcentration step and/or purification step, to a fermentation,hydrolysis, chemical treatment, catalytic treatment, polymerizationprocess, depolymerization process, degradation process, enzymatictreatment, manufacture of binder, manufacture of feed, manufacture offood or other suitable process or their combinations.

In one embodiment, a lignin fraction (7) comprising solids is recovered.The lignin fraction may be used as component in manufacturing a finalproduct. In one embodiment, the lignin fraction can be treated, e.g.purified, for further use. In one embodiment, the lignin fraction issupplied to a further processing. In one embodiment, the lignin fractionis supplied to a hydrolysis which may be selected from the groupconsisting of acid hydrolysis, supercritical hydrolysis and/orsubcritical hydrolysis and their combinations, or to a polymerizationprocess or to a depolymerization process or to a degradation process orto a chemical treatment or to a manufacture of a composite material orto a manufacture of binder, e.g. wood based binder, or to a manufactureof feed or to a manufacture of food or to a combustion process or toother suitable process or their combinations. The lignin fraction may besupplied directly to a hydrolysis, polymerization process,depolymerization process, degradation process, chemical treatment,manufacture of a composite material, manufacture of binder, manufactureof feed, manufacture of food, combustion process or other suitableprocess or their combinations, or alternatively via a suitable treatmentstep or an additional step, e.g. additional concentration step and/orpurification step, to a hydrolysis, polymerization process,depolymerization process, degradation process, chemical treatmentmanufacture of a composite material, manufacture of binder, manufactureof feed, manufacture of food, combustion process or other suitableprocess or their combinations.

In one embodiment, at least a part of lignin based material (5)comprising solids is recovered. The lignin based material may be used ascomponent in manufacturing a final product. In one embodiment, thelignin based material can be treated, e.g. purified, for further use. Inone embodiment, the lignin based material is supplied to a furtherprocessing. In one embodiment, the lignin based material is supplied toa hydrolysis which may be selected from the group consisting of acidhydrolysis, supercritical hydrolysis and/or subcritical hydrolysis andtheir combinations, or to a polymerization process or to adepolymerization process or to a degradation process or to a chemicaltreatment or to a manufacture of a composite material or to amanufacture of binder, e.g. wood based binder, or to a manufacture offeed or to a manufacture of food or to a combustion process or to othersuitable process or their combinations. The lignin based material may besupplied directly to a hydrolysis, polymerization process,depolymerization process, degradation process, chemical treatment,manufacture of a composite material, manufacture of binder, manufactureof feed, manufacture of food, combustion process or other suitableprocess or their combinations, or alternatively via a suitable treatmentstep or an additional step, e.g. additional concentration step and/orpurification step, to a hydrolysis, polymerization process,depolymerization process, degradation process, chemical treatment,manufacture of a composite material, manufacture of binder, manufactureof feed, manufacture of food, combustion process or other suitableprocess or their combinations.

In one embodiment, the liquid fraction (11) is recovered. The liquidfraction may be used as component in manufacturing a final product. Inone embodiment, the liquid fraction can be concentrated for further use.In one embodiment, the liquid fraction is supplied to a furtherprocessing. The liquid fraction may be supplied directly to afermentation, hydrolysis, chemical treatment, catalytic treatment,polymerization process, depolymerization process, degradation process,enzymatic process, manufacture of binder, manufacture of feed,manufacture of food or other suitable process or their combinations, oralternatively via a suitable treatment step or an additional step, e.g.additional concentration step and/or purification step, to afermentation, hydrolysis, chemical treatment, catalytic treatment,polymerization process, depolymerization process, degradation process,enzymatic process, manufacture of binder, manufacture of feed,manufacture of food or other suitable process or their combinations.

In one embodiment, the solid fraction (10) is formed from thelignocellulosic material (3 a,3 b). In one embodiment, at least a partof the solid fraction can be recovered and used as component inmanufacturing a final product. In one embodiment, the solid fraction issupplied to a further processing. The solid fraction may be supplieddirectly to a hydrolysis, polymerization process, depolymerizationprocess, degradation process, chemical treatment, manufacture of acomposite material, manufacture of binder, combustion process or othersuitable process or their combinations, or alternatively via a suitabletreatment step or an additional step, e.g. additional concentration stepand/or purification step, to a hydrolysis, polymerization process,depolymerization process, degradation process, chemical treatment,manufacture of a composite material, manufacture of binder, combustionprocess or other suitable process or their combinations.

In one embodiment, the soluble carbohydrate containing fraction (8) andthe liquid fraction (11) is combined partially or as a whole in order toform a liquid mixture. In one embodiment, the liquid mixture comprises1-99 w-% soluble carbohydrate containing fraction and 1-99 w-% liquidfraction, from the total weight of the soluble carbohydrate containingfraction and liquid fraction. The liquid mixture may be used ascomponent in manufacturing a final product. In one embodiment, theliquid mixture can be concentrated for further use. In one embodiment,the liquid mixture is supplied to a further processing. The liquidmixture may be supplied directly to a fermentation, hydrolysis, chemicaltreatment, catalytic treatment, polymerization process, depolymerizationprocess, degradation process, enzymatic treatment, manufacture ofbinder, manufacture of feed, manufacture of food or other suitableprocess or their combinations, or alternatively via a suitable treatmentstep or an additional step, e.g. additional concentration step and/orpurification step, to a fermentation, hydrolysis, chemical treatment,catalytic treatment, polymerization process, depolymerization process,degradation process, enzymatic treatment, manufacture of binder,manufacture of feed, manufacture of food or other suitable process ortheir combinations.

In one embodiment, water soluble matter is determined by a gravimetricwashing method. The determination by the gravimetric washing method maybe done as following: dry matter content (DM %) of raw material, e.g.the solid and soluble fraction, is measured at 60° C., the amount ofsolids remaining after heating the sample at 60° C. to constant weightis measured and dry matter content is calculated based on wet and dryweights. For washing about 10 g bone dry of the wet material underinvestigation is taken, weighted (exact weighed amount) and mixed withhot water (50° C.) in a vessel so that total amount is 200 g, themixture is mixed 20 s (Bamix Mono freehand food blender, ‘C’ blade,speed 1 (7000 rpm)), the mixture is soaked with soaking time 5 min, themixture is mixed 10 s (Bamix Mono freehand food blender, C′ blade, speed1 (7000 rpm)), mass of a dry filter paper is measured, the mixture isfiltered by means of Büchner (dia.125 mm) and the filter paper, aninward relief valve is closed when a cake is matt (dry) in whole, afiltrate is taken and the blender and vessel is washed with the filtrateand the filtrate is filtered again through the cake, the cake is washedthree times with hot water, a 100 g, so that suction effect ismaintained the whole time and washing water (100 g) is added when thecake is matt (dry) in whole, a foil dish is weighed, the cake with thefilter paper is dried in the foil dish, the dried cake (60° C.) with thefilter paper is weighed in the foil dish and mass of the filter paperand foil dish is subtracted from mass of the dried cake, filter paperand foil dish, and then soluble matter free solid, i.e. water insolublesolids (WIS) of wet material under investigation, can be determined.Water insoluble solids, WIS %, can be calculated: WIS %=(weight ofwashed and dried material, e.g. the cake)/(weight of the wet slurry forwashing, e.g. the raw material). Water soluble matter, WS %, of drymatter can be calculated: WS %=(dry matter (DM %) of the originalslurry, e.g. the raw material)−(water insoluble solids, WIS %).

In one embodiment, with high soluble material content (25-50% of totaldry matter soluble) of raw material, the lignin fraction (7) or solidfraction (10) contains soluble compounds below 20%, preferably below15%, more preferably below 9%, most preferably below 5%, by weight afterthe solid-liquid separation stage (6,9), measured by gravimetric washingmethod. In one embodiment, with lower soluble material content (below25% of total dry matter soluble) of raw material, the lignin fraction(7) or solid fraction (10) contains soluble compounds below 9%,preferably below 6%, more preferably below 3%, by weight after thesolid-liquid separation stage (6,9), measured by gravimetric washingmethod.

Particle size of the solid particles can be defined, e.g. by an opticalmeasurement device, such as Metso FS5 or Coulter LS230. In oneembodiment, particle size of the solid particles can be defined based onISO 16065-N or TAPPI T271. Fibre length of the solid particles can bedefined based on ISO 16065-N, when fibres are defined as material longerthan 0.2 mm. Fibre length of the solid particles can be defined based onTAPPI T271, when fibre length is 0.01 to 7.60 mm. In connection withMetso FS5, Lc means contour length, i.e. centerline fiber length, whichis fiber length measured from the fibers center line from one end toanother. Length-weighted Lc(l) means length-weighted fiber length whichis average fiber length measured from a fiber distribution weightedaccording to the TAPPI T271 standards. Weight-weighted Lc(w) meansweight-weighted fiber length which is likewise average fiber lengthmeasured from a fiber distribution weighted according to the TAPPI T271standards. Arithmetic Lc(n) means arithmetic mean which is calculatedfrom the population distribution of fibers. In this result averagelength is calculated from the length distribution. F1(1)% means lengthweighted distribution % (width>10 μm, length<0.2 mm). Fiber width ismeasured as integral value from the middle of the fiber to account fortapered ends.

In one embodiment, length-weighted particle length Lc(l) is below[(0.4)×(corresponding unrefined sulphate pulp fibre length)], in oneembodiment below [(0.3)×(corresponding unrefined sulphate pulp fibrelength)], in one embodiment below [(0.2)×(corresponding unrefinedsulphate pulp fibre length)], in one embodiment below[(0.1)×(corresponding unrefined sulphate pulp fibre length)].

In one embodiment, fine particle width (fraction 0-0.2 mm) is below[(0.7)×(corresponding unrefined sulphate pulp fibre length)], in oneembodiment below [(0.6)×(corresponding unrefined sulphate pulp fibrelength)], in one embodiment below [(0.5)×(corresponding unrefinedsulphate pulp fibre length)], in one embodiment below[(0.4)×(corresponding unrefined sulphate pulp fibre length)].

In one embodiment, the determination of particle size of the solidparticles in the cake needs proper sample preparation to disperse singleparticles to water. For dispersing about 10 g bone dry of the wetmaterial under investigation is taken and mixed with water (about 20°C.) in a vessel so that total amount is 200 g, the mixture is soakedwith soaking time 15 min, and the mixture is mixed 60 s (Bamix Monofreehand food blender, ‘C’ blade, speed 1 (7000 rpm)). After that thematerial is ready to determination specific preparation. In oneembodiment, to have more reliable picture of fine particles, shorterthan 0.2 mm, measurement is done by an optical measurement device, suchas Metso FS5, such way that material pass the detector only once, so itis not circulated back to detector. In one embodiment, the amount ofmeasured dry matter in one run is 1.6 g.

In one embodiment, the fine solid particles are fiber-like orindefinable particles with longest dimension shorter than 0.2 mmmeasured with optical Metso FS5 (fraction F1(l) of length weighted Lc(l)measurements and calculations). In one embodiment, the lignocellulosicmaterial (3 a,3 b) or solid fraction (10) of hardwood comprisesparticles with longest dimension shorter than 0.2 mm over 70%(F1(l)>70%), preferably over 80%, more preferably over 90% and mostpreferably over 95% by weight, defined by Metso FS5 (single pass run).In one embodiment, the lignocellulosic material (3 a,3 b) or solidfraction (10) of softwood comprises particles with longest dimensionshorter than 0.2 mm over 50% (F1(l)>50%), preferably over 60%, morepreferably over 70% and most preferably over 80% by weight, defined byMetso FS5 (single pass run). In one embodiment, the lignin fraction (7)comprises particles with longest dimension shorter than 0.2 mm over 70%(F1(l)>70%), preferably over 80%, more preferably over 90% and mostpreferably over 95% by weight, defined by Metso FS5 (single pass run).

In one embodiment, the lignocellulosic material (3 a,3 b) or solidfraction (10) comprises fine solid particles which are fiber-like orindefinable particles. The length weighted length Lc(l) is measuredbased TAPPI T271 standard includes all the particles detected andfilling the requirements of measurement. TAPPI T271 defines fiber lengthof material to have longest dimension from 0.01 to 7.60 mm.

In one embodiment, the lignocellulosic material (3 a,3 b) or solidfraction (10) comprises fine solid particles which are fiber-like orindefinable particles. The length weighted length Lc(l) is measured withMetso FS5 (single pass run), where Lc(l) is including also the particlesbelow 0.2 mm. The length weighted Lc(l)-value is 40% or less of thelength of corresponding unrefined sulphate pulp fibre length, preferably30% or less, more preferably 20% or less, most preferably 10% or less.And the width of the fine particle fraction of length weighted particles(Lc(l) fraction 0-0.2 mm) is 70% or less of width of the correspondingsulphate pulp fibre, preferably 60% or less, more preferably 50% orless, the most preferably 40% or less.

In one embodiment, the lignocellulosic material (3 a,3 b) or solidfraction (10) of hardwood comprises fine solid particles which arefiber-like or indefinable particles. The length weighted length Lc(l) ismeasured with Metso FS5 (single pass run), where Lc(l) is including alsothe particles below 0.2 mm. The length weighted Lc(l) fractions over 0.2mm fibre length is 50% or less, preferably 35% or less, more preferably20% or less, most preferably 5% or less.

In one embodiment, the lignocellulosic material (3 a,3 b) or solidfraction (10) of softwood comprises fine solid particles which arefiber-like or indefinable particles. The length weighted length Lc(l) ofsolid fraction is measured with Metso FS5 (single pass run), where Lc(l)is including also the particles below 0.2 mm. The length weighted Lc(l)fractions over 0.2 mm fibre length is 60% or less, preferably 45% orless, more preferably 30% or less, most preferably 15% or less. In oneembodiment, the lignocellulosic material (3 a,3 b) or its solid fraction(10) contains fine solid particles which comprise less than 90%, in oneembodiment less than 88%, particles with below 50 μm particle size,defined by Coulter LS230. In one embodiment, the lignocellulosicmaterial (3 a, 3 b) or its solid fraction (10) contains fine solidparticles which comprise 50-90%, in one embodiment 60-90%, and in oneembodiment 70-90%, particles with below 50 μm particle size, defined byCoulter LS230. In one embodiment, the lignocellulosic material (3 a,3 b)or solid fraction (10) comprises particles with equivalent circular areadiameter smaller than 50 μm over 50%, in one embodiment over 70%, andpreferably below 90% by weight, defined by Coulter LS230. In oneembodiment, the lignocellulosic material (3 a,3 b) or solid fraction(10) comprises solid particles which are fiber-like or indefinableparticles measured in water solution with a laser diffraction methodCoulter LS230, PIDS (Polarization Intensity Differential Scattering)including. In one embodiment, the lignocellulosic material (3 a,3 b) orsolid fraction (10) comprises particles with Mode equivalent circulararea diameter less than 300 μm, in one embodiment less than 200 μm, inone embodiment less than 100 μm, in one embodiment 50 μm, in oneembodiment less than 40 μm, and in one embodiment less than 30 μm, andpreferably over 18 μm, defined by Coulter LS230. Coulter LS230 is basedon a laser diffraction, and it measures particle size distributions bymeasuring the pattern of light scattered by the constituent particles inthe sample. Coulter LS230 comprises an optical module consisting of adiffraction component and PIDS (Polarization Intensity DifferentialScattering) assembly. The measuring range is 0.04-2000 μm so that themeasuring range is 0.4-2000 μm with the diffraction component and themeasuring range is 0.04-0.4 μm with the PIDS assembly.

The method and apparatus provide the liquid fraction, solid fraction,soluble carbohydrate containing fraction and lignin fraction with goodquality. Further, concentration and sugar content of the solublecarbohydrate containing fraction can be increased. Further, the recoveryof the soluble carbohydrate containing fraction can be increased andmore pure lignin fraction solids can be formed. The lignin fraction hasalso very high concentration of lignin and glucan and its hydratedproducts. In the method, a replacement washing is preferably used whichleads to further increase of the concentration of the soluble compoundsand increase purity of the lignin fraction. Further, post-treating costsof the soluble carbohydrate containing fraction can be decreased. Highconcentration is achieved with low energy consumption.

The present invention provides an industrially applicable, simple andaffordable way of making the pure lignin fraction and further thesoluble carbohydrate containing fraction. The method and apparatus areeasy and simple to realize as a production process. The method andapparatus are suitable for use in the manufacture of the differentlignin based fractions and sugar based fractions, and final productsfrom different starting materials.

EXAMPLES

The invention is described in more detail by the following examples withreference to accompanying drawings.

Example 1

In this example a lignin fraction and soluble carbohydrate containingfraction are produced from plant based raw material according to aprocess of FIG. 1.

The lignocellulosic material (3 a) is formed from plant based rawmaterial (1) by means of one pretreatment step (2 a), or alternativelyby means of two pretreatment steps (2 a,2 b). The plant based rawmaterial (1) can be treated by means of a hydrolysis and steam explosiontreatment in presence of a chemical agent, e.g. H₂SO₄, at thepretreatment stage. The lignocellulosic material (3 a) is conducted intoan enzymatic hydrolysis (4) for forming a lignin based material (5). Thelignin based material (5) is conducted into a solid-liquid separationstage (6) which comprises a separation device based on filtration orcentrifugal treatment. A soluble carbohydrate containing fraction (8)and a lignin fraction (7) are separated at the solid-liquid separationstage (6). The soluble carbohydrate containing fraction (8) isrecovered. A solid cake (7) containing lignin is removed from thesolid-liquid separation device and recovered.

Example 2

In this example a lignin fraction and soluble carbohydrate containingfraction are produced from plant based raw material according to aprocess of FIG. 2.

The lignocellulosic material A (3 a) is formed from plant based rawmaterial (1) by means of a pretreatment step (2 a). The plant based rawmaterial (1) can be treated by means of a hydrolysis and steam explosiontreatment in presence of a chemical agent, e.g. H₂SO₄, at thepretreatment stage. The lignocellulosic material A (3 a) is treated bymeans of a soaking (2 c) after the pretreatment step (2 a). Thelignocellulosic material B (3 b) from the soaking step (2 c) isconducted into an enzymatic hydrolysis (4) for forming a lignin basedmaterial (5). The lignin based material (5) is conducted into asolid-liquid separation stage (6) which comprises a separation devicebased on filtration or centrifugal treatment. A soluble carbohydratecontaining fraction (8) and a lignin fraction (7) are separated at thesolid-liquid separation stage (6). The soluble carbohydrate containingfraction (8) is recovered. A solid cake (7) containing lignin is removedfrom the solid-liquid separation device and recovered.

Example 3

In this example a lignin fraction and soluble carbohydrate containingfraction are produced from plant based raw material according to aprocess of FIG. 3.

The lignocellulosic material A (3 a) is formed from plant based rawmaterial (1) by means of a pretreatment step (2 a). The plant based rawmaterial (1) can be treated by means of a hydrolysis and steam explosiontreatment in presence of a chemical agent, e.g. H₂SO₄, at thepretreatment stage. The lignocellulosic material A (3 a) is treated bymeans of a soaking (2 c) after the pretreatment step (2 a). Thelignocellulosic material B (3 b) from the soaking step (2 c) isconducted a solid-liquid separation stage (9) which comprises aseparation device based on filtration or centrifugal treatment and inwhich a liquid fraction (11) and a solid fraction (10) are separatedbefore an enzymatic hydrolysis (4), and the solid fraction (10) isconducted into the enzymatic hydrolysis (4) for forming a lignin basedmaterial (5). The lignin based material (5) is conducted into a secondsolid-liquid separation stage (6) which comprises a separation devicebased on filtration or centrifugal treatment. A soluble carbohydratecontaining fraction (8) and a lignin fraction (7) are separated at thesolid-liquid separation stage (6). The soluble carbohydrate containingfraction (8) is recovered. A solid cake (7) containing lignin is removedfrom the solid-liquid separation device and recovered.

Example 4

In this example a lignin fraction and soluble carbohydrate containingfraction are produced from plant based raw material according to aprocess of FIG. 4.

The lignocellulosic material A (3 a) is formed from plant based rawmaterial (1) by means of two pretreatment steps (2 a,2 b). The plantbased raw material (1) can be treated by means of a hydrolysis and steamexplosion treatment in presence of a chemical agent, e.g. H₂SO₄, at thepretreatment stage. The lignocellulosic material A (3 a) is treated bymeans of a soaking (2 c) after the pretreatment steps (2 a,2 b). Thelignocellulosic material B (3 b) from the soaking step (2 c) isconducted a solid-liquid separation stage (9) which comprises aseparation device based on filtration or centrifugal treatment and inwhich a liquid fraction (11) and a solid fraction (10) are separatedbefore an enzymatic hydrolysis (4). In one embodiment, a part of liquidfraction which comprises soluble carbohydrates may be supplied outand/or recovered between pretreatment steps (2 a,2 b) or in connectionwith them. The solid fraction (10) is conducted into the enzymatichydrolysis (4) for forming a lignin based material (5). The lignin basedmaterial (5) is conducted into a second solid-liquid separation stage(6) which comprises a separation device based on filtration orcentrifugal treatment. A soluble carbohydrate containing fraction (8)and a lignin fraction (7) are separated at the solid-liquid separationstage (6). The soluble carbohydrate containing fraction (8) isrecovered. A solid cake (7) containing lignin is removed from thesolid-liquid separation device and recovered.

Example 5

In this example a concentrated liquid (11) and purified solid fraction(10) were produced.

Birch wood chips were pretreated in two-step dilute acid steam explosionprocess (2 a,2 b) to dissolve hemicellulose. The formed lignocellulosicmaterial (3 a) was mixed with hot water and stirred for a while in asoaking step (2 c). Then solid-liquid separation was done with OutotecLarox PF 0.1 pressure filter (9). Filtration area was 0.1 m². Amount ofwashing water was 1:1 (water:water insoluble solids in the cake) and3:1. Dry matter of original pretreated biomass was 65%, dry matter ofthe feed (3 b) in the first filtration (9) was 16%, and water insolublesolid content of that was 13%. Water insoluble solid content of the feedwas kept constant in filter press while dry matter of slurry wasincreased due to increased soluble material in slurry. Dry matter ofwashed cake was about 50%. Composition of the solid fraction, which isfurther washed in laboratory like in gravimetric washing method toremove all water soluble material, is presented in Table 1. The solidfraction was washed with water in order to remove residue solublecompounds, and after that the properties were determined.

To simulate the increase of concentration when all the washing filtrateof the process and some soluble carbohydrate containing filtrate offirst pressing was calculated to use as dilution water of next round,and again after second filtration the washing filtrate and some solublecarbohydrate containing filtrate of pressing was used in dilution ofthird filtration. In 1:1 washing case about 83% of dilution liquid wassoluble carbohydrate containing filtrate and in 3:1 case 48% of dilutionliquid was soluble carbohydrate containing filtrate. Washing efficiencywas calculated to be 83% (1:1) and 88% (3:1). Finally more than 70iteration rounds were done. Simulation of the example was done withmeasured soluble matter content of 18.4% of the pretreatedlignocellulosic material. The concentration of soluble matter containingfiltrate coming out of the process will reach level of 135 g/l incontinuous process with 1:1 washing and 99 g/l with 3:1 washing.

TABLE 1 Test Test Property Unit Method 1 2 Acid-insoluble lignin, %T-222 33.4 34.0 grav. Acid-soluble lignin, % T-UM 250 1.5 1.5 UV205Arabinose, acid hydrolysis, mg/g SCAN- 0.0 0.0 HPAE-PAD CM71 Rhamnose,acid mg/g SCAN- 0.0 0.0 hydrolysis, HPAE-PAD CM71 Galactose, acid mg/gSCAN- 0.0 0.0 hydrolysis, HPAE-PAD CM71 Glucose, acid mg/g SCAN- 599.3642.7 hydrolysis, HPAE-PAD CM71 Xylose, acid mg/g SCAN- 25.8 26.1hydrolysis, HPAE-PAD CM71 Mannose, acid mg/g SCAN- 0.0 0.0 hydrolysis,HPAE-PAD CM71 Carbohyrates, acid mg/g SCAN- 625.1 668.7 hydrolysis,HPAE-PAD, total CM71 FS5 Length weighted mm Determined 0.310 0.405 fiberlength Lc (1) ISO by Metso FS5 based on ISO 16065-N or TAPPI T271 FS5Fiber width μm 23.8 19.1 FS5 Fines % 99.5 99.1 FS5 Fines (Flakes) % 95.093.5 FS5 Fines (Fibrils) % 0.0 0.0 Population based mm 0.018 0.018particle length Lc (n) Length weighted particle mm 0.026 0.029 length Lc(1) Weight weighted particle mm 0.061 0.111 length Lc (w) FSS Fiberfractions % 99.5 99.0 0-0.2 mm FS5 Fiber fractions % 0.4 0.8 0.2-0.6 mmFS5 Fiber fractions % 0.0 0.1 0.6-1.2 mm FS5 Fiber fractions % 0.0 0.01.2-2.0 mm FS5 Fiber fractions % 0.0 0.0 2.0-3.2 mm FS5 Fiber fractions% 0.0 0.0 3.2-7.6 mm Particle width of fraction μm 4.3 4.4 0-0.2 mmParticle width of μm 25.0 19.0 fraction 0.2-0.6 mm Particle width of μm11.7 15.5 fraction 0.6-1.2 mm Particle width of μm 13.0 46.4 fraction1.2-2.0 mm Particle with of μm fraction 2.0-3.2 mm Particle width of μmfraction 3.2-7.6 mm FS5 Mass fractions % 88.7 87.0 0-0.2 mm FS5 Massfractions % 11.2 11.1 0.2-0.6 mm FS5 Mass fractions % 0.2 0.8 0.6-1.2 mmFS5 Mass fractions % 0.0 1.2 1.2-2.0 mm FS5 Mass fractions % 0.0 0.02.0-3.2 mm FS5 Mass fractions % 0.0 0.0 3.2-7.6 mm FS5 Number ofpictures pcs 639 644 (avg of 3) FS5 Number of particles pcs 117076106621 (avg of 3)

Example 6

In this example a liquid fraction (11) and solid fraction (10) wereproduced.

Eucalyptus wood chips were pretreated in one-step autohydrolysis andsteam explosion process with two different process conditions todissolve hemicellulose. The formed pretreated lignocellulosic materialswere washed with hot water in laboratory to remove most of the watersoluble compounds. These remaining, water soluble compound free solidswere measured with two different particle size analyzer. The results ofMetso FS5 and Coulter LS230 are presented in table 2 ‘two waterinsoluble solids of pretreated eucalyptus based lignocellulosicmaterials’. The results may be determined by standards of ISO 16065-N orTAPPI T271.

TABLE 2 Material Material Unit 1 2 FS5 Length weighted fiber mm 0.3320.462 length Lc (1) ISO FS5 Fiber width μm 16.2 21.8 FS5 Fines % 98.686.8 FS5 Fines (Flakes) % 94.6 66.9 FS5 Fines (Fibrils) % 0.0 0.0Population based particle mm 0.018 0.026 length Lc (n) Length weightedparticle mm 0.031 0.099 length Lc (1) Weight weighted particle mm 0.0990.383 length Lc (w) FS5 Fiber fractions 0-0.2 mm % 98.6 86.8 FS5 Fiberfractions 0.2-0.6 mm % 1.3 9.6 FS5 Fiber fractions 0.6-1.2 mm % 0.1 3.6FS5 Fiber fractions 1.2-2.0 mm % 0.0 0.0 FS5 Fiber fractions 2.0-3.2 mm% 0.0 0.0 FS5 Fiber fractions 3.2-7.6 mm % 0.0 0.0 Particle width offraction μm 5.9 7.9 0-0.2 mm Particle width of fraction μm 16.3 21.10.2-0.6 mm Particle width of fraction μm 15.4 23.6 0.6-1.2 mm Particlewidth of fraction μm 1.2-2.0 mm Particle with of fraction μm 2.0-3.2 mmParticle width of fraction μm 3.2-7.6 mm FS5 Mass fractions 0-0.2 mm %94.2 52.7 FS5 Mass fractions 0.2-0.6 mm % 5.7 32.3 FS5 Mass fractions0.6-1.2 mm % 0.2 15.0 FS5 Mass fractions 1.2-2.0 mm % 0.0 0.0 FS5 Massfractions 2.0-3.2 mm % 0.0 0.0 FS5 Mass fractions 3.2-7.6 mm % 0.0 0.0Coulter LS Particle size Mean μm 36.5 54.8 Coulter LS Particle sizeMedian μm 29.9 40.8 Coulter LS Particle size Mode μm 72.9 116.3 CoulterLS Particle size <50 μm % 70.6 57.0 Coulter LS Particle size <25 μm %43.4 32.6 Coulter LS Particle size <10 μm % 19.2 11.6 Coulter LSParticle size <5 μm % 10.5 6.5 Coulter LS Particle size <2 μm % 4.3 2.8Coulter LS Particle size <1 μm % 1.9 1.1 Coulter LS Particle size <0.5μm % 0.8 0.3 Coulter LS Particle size <0.3 μm % 0.4 0.1

Example 7

In this example, liquid and solid fractions were produced, and theiruses in an enzymatic hydrolysis were examined.

Birch wood chips were pretreated in a dilute acid steam explosionprocess (2 a) to dissolve hemicellulose for forming a lignocellulosicmaterial (3 a).

The lignocellulosic material (3 a) was soaked in a soaking step (2 c)for forming a lignocellulosic material (3 b). During the soaking,residence time was 24 hours, temperature was about 50° C., andconsistency was 28%.

The treated lignocellulosic material (3 b) was supplied to asolid-liquid separation device (9). The separation device was a decantercentrifuge in experiments PTB1, PTB2 and PTB3, and the separation devicewas a pressure filter in experiment PTB4.

The solid samples (PTB1, PTB2, PTB3, PTB4) of the treated biomass weretaken after separation stage (9). The results are presented in Table 3.

Further, the solid sample PTB2, taken after separation stage (9), wasdiluted to level of 15% total solids for an enzymatic hydrolysis (4) inlaboratory scale. Mixing of slurry was good, and 5% enzyme/total solidswas used in the experiment. Glucose yield after 72 hours was 80%.

Further, the solid sample PTB1, taken after separation stage (9), wasdiluted. It was observed that PTB1 was not possible to mix in thelaboratory experiment at total solids level of 13% or higher, and theenzymatic hydrolysis was not possible to do.

TABLE 3 Unit PTB1 PTB2 PTB3 PTB4 FS5 Length mm 1.399 1.665 0.500 0.764weighted fiber length Lc (1) ISO FS5 Fiber width μm 21.0 21.4 20.0 28.1FS5 Fines % 98.3 97.8 99.2 98.7 FS5 Fiber fractions % 98.3 97.8 99.298.7 0-0.2 mm FS5 Fiber fractions % 0.90 1.00 0.60 0.70 0.2-0.6 mm FS5Fiber fractions % 0.20 0.40 0.10 0.30 0.6-1.2 mm FS5 Fiber fractions %0.10 0.10 0.10 0.30 1.2-2.0 mm FS5 Fiber fractions % 0.20 0.20 0.00 0.002.0-3.2 mm FS5 Fiber fractions % 0.30 0.50 0.00 0.00 3.2-7.6 mm FS5Number pcs 114084 119703 107226 120079 of particles FS5 Number of fiberspcs 114082 119690 107219 120067 FS5 Fines (Flakes) % 93.8 90.0 96.4 92.1Population based mm 0.020 0.019 0.018 0.017 particle length Lc (n)Length weighted mm 0.069 0.065 0.029 0.031 particle length Lc (1) Weightweighted mm 1.538 1.852 0.190 0.444 particle length Lc (w) Particlewidth of μm 5.2 4.3 4.4 4.3 fraction 0-0.2 mm Particle width of μm 18.921.0 26.7 23.1 fraction 0.2-0.6 mm Particle width of μm 18.1 14.9 24.520.2 fraction 0.6-1.2 mm Particle width of μm 29.2 18.1 15.4 37.5fraction 1.2-2.0 mm Particle with of μm 22.9 21.0 23.1 16.6 fraction2.0-3.2 mm Particle width of μm 24.1 26.6 13.3 fraction 3.2-7.6 mm FS5Mass fractions % 73.7 72.1 82.7 80.9 0-0.2 mm FS5 Mass fractions % 8.413.0 14.1 11.9 0.2-0.6 mm FS5 Mass fractions % 3.3 1.7 2.5 2.1 0.6-1.2mm FS5 Mass fractions % 6.1 2.8 0.2 4.7 1.2-2.0 mm FS5 Mass fractions %4.6 3.5 0.5 0.3 2.0-3.2 mm FS5 Mass fractions % 3.9 6.9 0.0 0.2 3.2-7.6mm Coulter LS Particle μm 20.3 23.8 29.4 28.6 size Mean Coulter LSParticle μm 15.9 18.4 22.1 21.1 size Median Coulter LS Particle μm 16.426.1 28.7 28.7 size Mode Coulter LS Particle % 93.8 87.7 80.2 80.4 size<50 μm Coulter LS Particle % 69.8 62.0 54.9 56.2 size <25 μm Coulter LSParticle % 30.6 28.4 21.9 24.8 size <10 μm Coulter LS Particle % 11.611.9 8.4 10.2 size <5 μm Coulter LS Particle % 1.9 2.2 1.5 1.8 size <2 mCoulter LS Particle % 0.1 0.1 0.1 0.1 size <1 μm Coulter LS % 0.0 0.00.0 0.0 Particle size <0.5 μm Coulter LS % 0.0 0.0 0.0 0.0 Particle size<0.3 μm Coulter LS Particle m2/g 0.61 0.59 0.48 0.53 size Spesificsurface area Brookfield viscosity mPas 19500 6233 10 rpm vane spindle45° C., 15% total solids

Example 8

In this example, viscosity of the lignocellulosic material was measured.The lignocellulosic material was according to example 7 after separation(9).

The viscosity was measured at 10, 15 and 20% dry matter content by meansof Brookfield viscosity device at 45° C. with 10 rpm and spindel type“Vane”. The sample size in the measurement was 300 ml. Sample A had goodmixing properties. Sample B had poor mixing properties in mechanicallyagitated vessel where mixing was done with pitched-blade turbine (45°)type of impellers.

The results from the viscosity measurements are presented in FIG. 5. Itwas observed that the lignocellulosic material with viscosity below18000 mPas, at 15% dry matter content, is suitable material for anenzymatic hydrolysis and a manufacture of lignin.

The method and apparatus are suitable in different embodiments to beused for producing the most different kinds of lignin and solublecarbohydrate based fractions from different plant based raw materials.

The invention is not limited merely to the example referred to above;instead many variations are possible within the scope of the inventiveidea defined by the claims.

1. A method for treating plant based raw material with an enzymatichydrolysis, in which the plant based raw material is treated to formlignocellulosic material and the lignocellulosic material or itsfraction is conducted into the enzymatic hydrolysis, wherein the methodcomprises at least one treatment stage in which the plant based rawmaterial is treated so that the lignocellulosic material contains over80% fine solid particles which are fiber-like or indefinable particlessmaller than 0.2 mm, defined by an optical measurement device, thelignocellulosic material or at least one fraction of the lignocellulosicmaterial is supplied into the enzymatic hydrolysis for forming a ligninbased material, and at least one solid-liquid separation stage after theenzymatic hydrolysis into which the lignin based material is suppliedand in which a lignin fraction and a soluble carbohydrate containingfraction are separated.
 2. The method according to claim 1, wherein thetreatment stage comprises at least one pretreatment step which isselected from the group consisting of physical treatment, such asmilling, extrusion, microwave treatment, ultrasound treatment and freezetreatment, chemical treatment, such as acid treatment, alkalinetreatment, ionic liquid treatment, organosolv treatment and ozonolysis,physico-chemical treatment, such as steam explosion treatment, ammoniafiber explosion treatment, CO₂ explosion treatment, liquid hot watertreatment and wet oxidation, biological treatment and theircombinations.
 3. The method according to claim 2, wherein the plantbased raw material is treated by means of a steam explosion treatment atthe pretreatment step.
 4. The method according to claim 2, wherein theplant based raw material is treated by means of a steam explosiontreatment in presence of a chemical agent at the pretreatment step. 5.The method according to claim 4, wherein the chemical agent is anon-alkaline agent.
 6. The method according to claim 4, wherein thechemical agent is an acid.
 7. The method according to claim 1, whereinthe lignocellulosic material is treated by means of a soaking.
 8. Themethod according to claim 1, wherein the lignocellulosic material isdiluted for the soaking.
 9. The method according to claim 1, wherein thelignocellulosic material contains fine solid particles from which over80% are smaller than 0.2 mm, defined by Metso FS5.
 10. The methodaccording to claim 1, wherein the lignocellulosic material comprisesfine solid particles which have particle size Mode between 18-300 μm,defined by Coulter LS230.
 11. The method according to claim 1, whereinthe viscosity of the lignocellulosic material is below 18000 mPas at 15%dry matter content, measured by Brookfield viscosity device at 45° C.with 10 rpm and spindel type “Vane”.
 12. The method according to claim1, wherein the method comprises more than one solid-liquid separationstages.
 13. The method according to claim 1, wherein the lignocellulosicmaterial is conducted a solid-liquid separation stage in which a liquidfraction and a solid fraction are separated before the enzymatichydrolysis, and the solid fraction is conducted into the enzymatichydrolysis.
 14. The method according to claim 1, wherein thesolid-liquid separation is made by means of filtration, centrifugaltreatment or their combinations.
 15. The method according to claim 1,wherein the solid-liquid separation stage comprises a washing in which adisplacement washing is carried out with small amount clean water inwhich ratio of washing water to solid is below
 6. 16. The methodaccording to claim 1, wherein the plant based raw material compriseswood based material or a mixture comprising wood based material.
 17. Anapparatus for treating plant based raw material with an enzymatichydrolysis, in which the apparatus comprises a treatment device and anenzymatic hydrolysis device, wherein the apparatus comprises at leastone treatment device in which the plant based raw material is treated toform lignocellulosic material so that the lignocellulosic materialcontains over 80% fine solid particles which are fiber-like orindefinable particles smaller than 0.2 mm, defined by an opticalmeasurement device, at least one enzymatic hydrolysis device in which alignin based material is formed from the lignocellulosic material or atleast one fraction of the lignocellulosic material, at least onesolid-liquid separation device after the enzymatic hydrolysis device inwhich a lignin fraction and a soluble carbohydrate containing fractionis separated from lignin based material, and at least one feeding devicefor feeding the plant based raw material into the treatment device. 18.The apparatus according to claim 17, wherein the apparatus comprisesmore than one solid-liquid separation devices.
 19. The apparatusaccording to claim 17, wherein the apparatus comprises at least onesolid-liquid separation device for separating a liquid fraction and asolid fraction.
 20. The apparatus according to claim 17, wherein theapparatus comprises at least one filtration device and/or centrifugaldevice as the solid-liquid separation device.
 21. The apparatusaccording to claim 17, wherein the apparatus comprises a means for asteam explosion.
 22. The apparatus according to claim 17, wherein theapparatus comprises a soaking device.
 23. A soluble carbohydratecontaining fraction obtainable by the method according to claim
 1. 24. Alignin fraction obtainable by the method according to claim
 1. 25. Alignin based material fraction obtainable by the method according toclaim
 1. 26. A liquid fraction obtainable by the method according toclaim
 1. 27. A solid fraction obtainable by the method according toclaim
 1. 28. A Use of the soluble carbohydrate containing fractionobtainable by the method according to claim 1, wherein the solublecarbohydrate containing fraction is used as a source material in afermentation, hydrolysis, chemical treatment, catalytic treatment,polymerization process, depolymerization process, degradation process,enzymatic treatment, manufacture of binder, manufacture of feed,manufacture of food or other suitable process or their combinations. 29.A use of the lignin fraction obtainable by the method according to claim1, wherein the lignin fraction is used as a source material in ahydrolysis, polymerization process, depolymerization process,degradation process, chemical treatment, manufacture of a compositematerial, manufacture of binder, manufacture of feed, manufacture offood, combustion process or other suitable process or theircombinations.
 30. A use of the lignin based material obtainable by themethod according to claim 1, wherein the lignin based material is usedas a source material in a hydrolysis, polymerization process,depolymerization process, degradation process, chemical treatment,manufacture of a composite material, manufacture of binder, manufactureof feed, manufacture of food, combustion process or other suitableprocess or their combinations.
 31. A use of the liquid fractionobtainable by the method according to claim 1, wherein the liquidfraction is used as a source material in a fermentation, hydrolysis,chemical treatment, catalytic treatment, polymerization process,depolymerization process, degradation process, enzymatic process,manufacture of binder, manufacture of feed, manufacture of food or othersuitable process or their combinations.
 32. A use of the solid fractionobtainable by the method according to claim 1, wherein the solidfraction is used as a source material in a hydrolysis, polymerizationprocess, depolymerization process, degradation process, chemicaltreatment, manufacture of a composite material, manufacture of binder,combustion process or other suitable process or their combinations. 33.A use of the liquid mixture comprising soluble carbohydrate containingfraction and liquid fraction obtainable by the method according to claim1, wherein the liquid mixture is used as a source material in afermentation, hydrolysis, chemical treatment, catalytic treatment,polymerization process, depolymerization process, degradation process,enzymatic treatment, manufacture of binder, manufacture of feed,manufacture of food or other suitable process or their combinations.